A cell for in situ observation of self-assembled nanostructured materials in high-pressure fluids, including supercritical carbon dioxide, has been constructed and tested. The compact cell can be used for simultaneous small-angle x-ray scattering, laser light scattering, visual observation, and some other types of spectroscopic measurements. The light scattering plane is normal to the x-ray scattering plane with the optical axis and the x-ray axis being perpendicular to each other. The scattering is detected at the intersection of the light and x-ray beams, and thus one effectively probes the same scattering volume. Some preliminary experimental results for the micellar self-assembly of a fluorinated block copolymer in supercritical carbon dioxide are presented.
REFERENCES
1.
M. A. MuHugh and V. Krukonis, Supercritical Fluids Extraction: Principles and Practice, 2nd ed. (Butterworth-Heinemann, Woburn, MA, 1994).
2.
See, for example,
J. L.
Kendall
, D. A.
Canelas
, J. L.
Young
, and J. M.
DeSimone
, Chem. Rev.
99
, 543
(1999
), and references cited therein.3.
K. A.
Arora
, A. J.
Lesser
, and T. J.
McCarthy
, Macromolecules
31
, 4614
(1998
).4.
C. M.
Stafford
, T. P.
Russell
, and T. J.
McCarthy
, Macromolecules
32
, 7610
(1999
).5.
6.
7.
Y. P.
Handa
, P.
Kruus
, and M.
ONeill
, J. Polym. Sci., Part B: Polym. Phys.
34
, 2635
(1996
).8.
T. Hashimoto, M. Shibayama, M. Fujimura, and H. Kawai, Block Copolymers: Science and Technology (Harwood Academic, London, 1983).
9.
J. L.
Fulton
, J. P.
Blitz
, J. M.
Tingey
, and R. D.
Smith
, J. Phys. Chem.
93
, 4189
(1989
).10.
R. D.
Smith
, J. L.
Fulton
, J. P.
Blitz
, and J. M.
Tingey
, J. Phys. Chem.
94
, 781
(1990
).11.
12.
J. M.
Ritter
, A. M. F.
Palavvra
, C. P. C.
Kao
, and M. E.
Paulaitis
, Fluid Phase Equilibria
55
, 173
(1990
).13.
E. W.
Kaler
, J. F.
Billman
, J. L.
Fulton
, and R. D.
Smith
, J. Phys. Chem.
95
, 458
(1991
).14.
J. L.
Fulton
, D. M.
Pfund
, R. D.
Smith
, N. F.
Carnaham
, L.
Quintero
, M.
Capel
, and K.
Leontaritis
, Langmuir
9
, 2035
(1993
).15.
J.
Kojima
, M.
Takenaka
, Y.
Nakayama
, and T.
Hashimoto
, Rev. Sci. Instrum.
66
, 4066
(1995
).16.
J. L.
Fulton
, D. M.
Pfund
, J. B.
McClain
, T. J.
Romack
, E. E.
Maury
, J. R.
Combes
, E. T.
Samulski
, and J. M.
DeSimone
, Langmuir
11
, 4241
(1995
).17.
R. G.
Zielinski
, M. E.
Paulaitis
, and E. W.
Kaler
, Rev. Sci. Instrum.
67
, 2612
(1996
).18.
D.
Chillura-Martino
, R.
Triolo
, J. B.
McClain
, J. R.
Combes
, D. E.
Betts
, D. A.
Canelas
, J. M.
DeSimone
, E. T.
Samulski
, H. D.
Cochran
, J. D.
Londono
, and G. D.
Wignall
, J. Mol. Struct.
383
, 3
(1996
).19.
J. B.
McClain
, D. E.
Betts
, D. A.
Canelas
, E. T.
Samulski
, J. M.
DeSimone
, J. D.
Londono
, H. D.
Cochran
, G. D.
Wignall
, D.
Chillura-Martino
, and R.
Triolo
, Science
274
, 2049
(1996
).20.
J. B.
McClain
, D.
Londono
, J. R.
Combes
, T. J.
Romack
, D. A.
Canelas
, D. E.
Betts
, G. D.
Wignall
, E. T.
Samulsli
, and J. M.
DeSimone
, J. Am. Chem. Soc.
118
, 917
(1996
).21.
S.
Zhou
, B.
Chu
, and H. S.
Dhadwal
, Rev. Sci. Instrum.
69
, 1955
(1998
).22.
E.
Buhler
, A. V.
Dobrynin
, J. M.
DeSimone
, and M.
Rubinstein
, Macromolecules
31
, 7347
(1998
).23.
24.
L.
Liu
, Z.
Cheng
, K.
Inomata
, S.
Zhou
, and B.
Chu
, Macromolecules
32
, 5836
(1999
).25.
F.
Triolo
, A.
Triolo
, R.
Triolo
, J. D.
Londono
, G. D.
Wignall
, J. B.
McClain
, D. E.
Betts
, S.
Wells
, E. T.
Samulski
, and J. M.
DeSimone
, Langmuir
16
, 416
(2000
).26.
W. F. Sherman and A. A. Stadtmuller, Experimental Techniques in High-Pressure Research (Wiley, New York, 1987).
27.
M.
Ji
, X.
Chen
, C. M.
Wai
, and J. L.
Fulton
, J. Am. Chem. Soc.
121
, 2631
(1999
).28.
S.
Yang
, J.
Wang
, K.
Ogino
, S.
Valiyaveettil
, and C. K.
Ober
, Chem. Mater.
1
, 33
(2000
).29.
O. Glatter and O. Kratky, Small Angle X-ray Scattering (Academic, London, 1982).
30.
31.
D. M.
Pfund
, T. S.
Zemanian
, J. C.
Linehan
, J. L.
Fulton
, and C. R.
Yonker
, J. Phys. Chem.
98
, 11846
(1994
).32.
N.
Sakamoto
, T.
Hashimoto
, C. D.
Han
, D.
Kim
, and N. Y.
Vaidya
, Macromolecules
30
, 1621
(1997
).33.
34.
J. M.
DeSimone
, X.
Guan
, and C. S.
Elsbernd
, Science
257
, 945
(1992
).35.
36.
T.
Hoefling
, D.
Sofesky
, M.
Reid
, and E.
Beckmen
, J. Supercrit. Fluids
5
, 237
(1992
).37.
A. Gunier and G. Fournet, Small-Angle Scattering of X Rays (Wiley, London, 1955).
38.
39.
40.
41.
B. Chu, Laser Light Scattering, 2nd ed. (Academic, New York, 1991).
42.
B. J. Berne and R. Pecora, Dynamic Light Scattering (Kreiger, Malabar, FL, 1990).
43.
44.
K. Stephan and K. Lucas, Viscosity of Dense Fluids (Plenum, New York, 1979).
45.
G. J.
Besserer
and D. B.
Robinson
, J. Chem. Eng. Data
18
, 137
(1973
).46.
S. Angus, B. Armstrong, and K. M. de Reuck, International Thermodynamic Tables of the Fluid State Carbon Dioxide (Pergamon, London, 1973).
This content is only available via PDF.
© 2001 American Institute of Physics.
2001
American Institute of Physics
You do not currently have access to this content.
